ASTM D4922-21
(Test Method)Standard Test Method for Determination of Radioactive Iron in Water
Standard Test Method for Determination of Radioactive Iron in Water
SIGNIFICANCE AND USE
5.1 Fe-55 is formed in reactor coolant systems of nuclear reactors by activation of stable iron. The 55Fe is not completely removed by waste processing systems and some is released to the environment by means of normal waste liquid discharges. Power plants are required to monitor these discharges for 55Fe as well as other radionuclides.
5.2 This technique effectively removes other activation and fission products such as isotopes of iodine, zinc, manganese, cobalt, and cesium by the addition of hold-back carriers and an anion exchange technique. The fission products (zirconium-95 and niobium-95) are selectively eluted with hydrochloric-hydrofluoric acid washes. The iron is finally separated from Zn+2 by precipitation of FePO4 at a pH of 3.0.
SCOPE
1.1 This test method covers the determination of 55Fe in the presence of 59Fe by liquid scintillation counting. The a-priori minimum detectable concentration for this test method is 7.4 Bq/L.2
1.2 This test method was developed principally for the quantitative determination of 55Fe. However, after proper calibration of the liquid scintillation counter with reference standards of each nuclide, 59Fe may also be quantified.
1.3 This test method was used successfully with Type III reagent water conforming to Specification D1193. It is the responsibility of the user to ensure the validity of this test method for waters of untested matrices.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 9.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4922 − 21
Standard Test Method for
1
Determination of Radioactive Iron in Water
This standard is issued under the fixed designation D4922; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D2777Practice for Determination of Precision and Bias of
55
Applicable Test Methods of Committee D19 on Water
1.1 This test method covers the determination of Fe in the
59 D3370Practices for Sampling Water from Flowing Process
presence of Fe by liquid scintillation counting. The a-priori
Streams
minimum detectable concentration for this test method is 7.4
2 D5847Practice for Writing Quality Control Specifications
Bq/L.
for Standard Test Methods for Water Analysis
1.2 This test method was developed principally for the
D7282Practice for Setup, Calibration, and Quality Control
55
quantitative determination of Fe. However, after proper cali-
of Instruments Used for Radioactivity Measurements
bration of the liquid scintillation counter with reference stan-
D7902Terminology for Radiochemical Analyses
59
dards of each nuclide, Fe may also be quantified.
3. Terminology
1.3 This test method was used successfully with Type III
reagent water conforming to Specification D1193.Itisthe
3.1 Definitions—For definitions of terms used in this test
responsibility of the user to ensure the validity of this test
method, refer to Terminologies D1129 and D7902. For terms
method for waters of untested matrices.
not defined in this test method or in Terminologies D1129 or
4
D7902, refer to other published glossaries.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4.1 This test method describes the effective separation of
mine the applicability of regulatory limitations prior to use.
iron from the interfering cations of manganese, cobalt,
For a specific hazard statement, see Section 9.
zirconium, niobium, and cesium by anion exchange using acid
1.5 This international standard was developed in accor-
washes of various molarities. Subsequent elution of the iron is
dance with internationally recognized principles on standard-
followed by phosphate precipitation to remove any residual
ization established in the Decision on Principles for the
zinc.The iron phosphate precipitate is dissolved in phosphoric
Development of International Standards, Guides and Recom-
acidandwaterandmixedwithliquidscintillationcocktail.The
mendations issued by the World Trade Organization Technical
chemical yield is determined by the recovery of iron carrier
Barriers to Trade (TBT) Committee.
using atomic absorption spectrophotometry.Alternatively, any
procedure described in Test Methods D1068 may be used, but
2. Referenced Documents
this will need to be validated by the user prior to reporting
3
sample results.
2.1 ASTM Standards:
D1068Test Methods for Iron in Water
5. Significance and Use
D1129Terminology Relating to Water
D1193Specification for Reagent Water 5.1 Fe-55 is formed in reactor coolant systems of nuclear
55
reactorsbyactivationofstableiron.The Feisnotcompletely
removed by waste processing systems and some is released to
1
the environment by means of normal waste liquid discharges.
This test method is under the jurisdiction ofASTM Committee D19 on Water
55
andisthedirectresponsibilityofSubcommitteeD19.04onMethodsofRadiochemi-
Power plants are required to monitor these discharges for Fe
cal Analysis.
as well as other radionuclides.
Current edition approved Dec. 15, 2021. Published May 2022. Originally
ɛ1
approved in 1989. Last previous edition approved in 2016 as D4922–09 (2016) .
5.2 This technique effectively removes other activation and
DOI: 10.1520/D4922-21.
fission products such as isotopes of iodine, zinc, manganese,
2
Currie, L., “Limits for Qualitative Detection and Quantitative Determination,”
Analytical Chemistry, Vol. 40, 1968, pp. 586–593.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM “American National Standard Glossary of Terms,” Nuclear Science and
Standards volume information, refer to the standard’s Document Summary page on Technology (ANSI N1.1), American National Standards Institute, 1430 Broadway,
the ASTM website. New York, NY 10018.
Copyright © ASTM I
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D4922 − 09 (Reapproved 2016) D4922 − 21
Standard Test Method for
1
Determination of Radioactive Iron in Water
This standard is issued under the fixed designation D4922; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1
ε NOTE—Editorial corrections were made to 5.1 in January 2016.
1. Scope
55 59
1.1 This test method covers the determination of Fe in the presence of Fe by liquid scintillation counting. The a-priori
2
minimum detectable concentration for this test method is 7.4 Bq/L.
55
1.2 This test method was developed principally for the quantitative determination of Fe. However, after proper calibration of the
59
liquid scintillation counter with reference standards of each nuclide, Fe may also be quantified.
1.3 This test method was used successfully with Type III reagent water conforming to Specification D1193. It is the responsibility
of the user to ensure the validity of this test method for waters of untested matrices.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 9.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
3
2.1 ASTM Standards:
D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Flowing Process Streams
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
D7282 Practice for Setup, Calibration, and Quality Control of Instruments Used for Radioactivity Measurements
D7902 Terminology for Radiochemical Analyses
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemical
Analysis.
Current edition approved Jan. 1, 2016Dec. 15, 2021. Published January 2016May 2022. Originally approved in 1989. Last previous edition approved in 20092016 as
ɛ1
D4922 – 09.D4922 – 09 (2016) . DOI: 10.1520/D4922-09R16E01.10.1520/D4922-21.
2
Currie, L., “Limits for Qualitative Detection and Quantitative Determination,” Analytical Chemistry, Vol. 40, 1968, pp. 586–593.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D4922 − 21
FIG. 1 Percent of Total Radionuclide Activity Removed Per Acid Wash
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to TerminologyTerminologies D1129 and D7902. For terms
4
not defined in this test method or in TerminologyTerminologies D1129 or D7902, refer to other published glossaries.
4. Summary of Test Method
4.1 This test method describes the effective separation of iron from the interfering cations of manganese, cobalt, zirconium,
niobium, and cesium by anion exchange using acid washes of various molarities. Subsequent elution of the iron is followed by
phosphate precipitation to remove any residual zinc. The iron phosphate precipitate is dissolved in phosphoric acid and water and
mixed with liquid scintillation cocktail. The chemical yield is determined by the recovery of iron carrier using atomic absorption
spectrophotometry. Alternatively, any procedure described in Test Methods D1068 may be used, but this will need to be validated
by the user prior to reporting sample results.
5. Significance and Use
55
5.1 Fe-55 is formed in reactor coolant sys
...
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